EP1088006B1 - Procede post-reacteur permettant de traiter des polymeres prepares par polymerisation en phase gazeuse en presence d'un materiau particulaire inerte - Google Patents

Procede post-reacteur permettant de traiter des polymeres prepares par polymerisation en phase gazeuse en presence d'un materiau particulaire inerte Download PDF

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Publication number
EP1088006B1
EP1088006B1 EP99930248A EP99930248A EP1088006B1 EP 1088006 B1 EP1088006 B1 EP 1088006B1 EP 99930248 A EP99930248 A EP 99930248A EP 99930248 A EP99930248 A EP 99930248A EP 1088006 B1 EP1088006 B1 EP 1088006B1
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EP
European Patent Office
Prior art keywords
polymer
particulate material
polymer particles
inert particulate
product
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Expired - Lifetime
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EP99930248A
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German (de)
English (en)
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EP1088006A1 (fr
Inventor
Ronald Steven Eisinger
Fathi David Hussein
David Nunn Jones
Ronald Irvin Raether
David Merrill Rebhan
Joseph Patrick Welch
Gary Harry Williams
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Union Carbide Chemicals and Plastics Technology LLC
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Union Carbide Chemicals and Plastics Technology LLC
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    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F210/00—Copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond
    • C08F210/16—Copolymers of ethene with alpha-alkenes, e.g. EP rubbers
    • C08F210/18—Copolymers of ethene with alpha-alkenes, e.g. EP rubbers with non-conjugated dienes, e.g. EPT rubbers
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
    • B01J8/18—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles
    • B01J8/1818—Feeding of the fluidising gas
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F136/00—Homopolymers of compounds having one or more unsaturated aliphatic radicals, at least one having two or more carbon-to-carbon double bonds
    • C08F136/02—Homopolymers of compounds having one or more unsaturated aliphatic radicals, at least one having two or more carbon-to-carbon double bonds the radical having only two carbon-to-carbon double bonds
    • C08F136/04—Homopolymers of compounds having one or more unsaturated aliphatic radicals, at least one having two or more carbon-to-carbon double bonds the radical having only two carbon-to-carbon double bonds conjugated
    • C08F136/06—Butadiene
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F136/00—Homopolymers of compounds having one or more unsaturated aliphatic radicals, at least one having two or more carbon-to-carbon double bonds
    • C08F136/02—Homopolymers of compounds having one or more unsaturated aliphatic radicals, at least one having two or more carbon-to-carbon double bonds the radical having only two carbon-to-carbon double bonds
    • C08F136/04—Homopolymers of compounds having one or more unsaturated aliphatic radicals, at least one having two or more carbon-to-carbon double bonds the radical having only two carbon-to-carbon double bonds conjugated
    • C08F136/08—Isoprene
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
    • C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
    • C08F220/42—Nitriles
    • C08F220/44—Acrylonitrile
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F6/00—Post-polymerisation treatments
    • C08F6/001—Removal of residual monomers by physical means
    • C08F6/005—Removal of residual monomers by physical means from solid polymers
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K3/00—Materials not provided for elsewhere
    • C09K3/14—Anti-slip materials; Abrasives
    • C09K3/1409—Abrasive particles per se

Definitions

  • a partial pressure slightly above to slightly below that is, for example, + 10°C for low boiling monomers
  • a readily condensable monomer e.g. butadiene or isoprene
  • the above-enumerated sticky elastomeric material having been produced as non-sticky polymers using one or more inert particulate materials, are dusty and contain loosely attached fines (inert particulate material or inert particulate material mixed with a small amount of polymer) on their surface.
  • the surfaces of the polymer particles are diffuse and have small carbon black attachments or inert particulate materials attachments, distributed evenly around the polymer particles.
  • the amount of loose inert particulate material (e.g., carbon black) between polymer particles is a function of the overall inert particulate material level.
  • a 200-mesh sieve and pan are installed under the 120-mesh sieve as normal, and the entire assembly re-installed in the Rotap apparatus.
  • the Rotap is started and run for times ranging from 5 and 10 minutes. Fines levels are then quantified, and the increase in fines from the ball bearing attrition test calculated by subtracting the initial fines levels. This Rotap test procedure is the preferred method for determining fines level or fines attrition.
  • Product receiving vessels are commercially available and can include, for example, Day® or Natta® mixers or a settled bed with bottom discharge. Such holding/receiving tanks can include stirring means such as paddles, revolving screw agitators, and/or blades though these are not required.
  • the EPDM is contacted with nitrogen or another inert gas (e.g., argon, carbon dioxide, a saturated C 1 -C 12 hydrocarbon such as ethane, propane, butane, isopentane, etc.).
  • nitrogen is heated to approximately 70°C, but can range from 55 to 120°C.
  • Nitrogen and unreacted monomer(s) e.g., propylene
  • the unreacted monomer(s) can be, and is/are preferably, recycled to the reactor.
  • the elastomer exits the product holding/receiving tank continuously (including semi-continuously) or batchwise, preferably continuously.
  • the amount of inert particulate material (e.g., carbon black) employed during the gas phase polymerization ranges from 6 to 10 phr.
  • the amounts are may be somewhat higher.
  • a reactor was operated at 40 °C to produce EPM product using V(AcAc) 3 catalyst with DEAC-TEAL (5:1 mole ratio) as co-catalyst and ETCA as promoter at an average production rate of 36,3 kg/h (80 pounds per hour).
  • the EPM product had a propylene content of 34.9 to 38.7 wt %; trace ENB content of 0.3 wt %; and a 54.5 to 75.9 Mooney viscosity.
  • Carbon black was fed continuously to the reactor resulting in a carbon level of 29.4 phr (parts per hundred parts rubber) for case 5a and 14.3 phr for case 5b.
  • the product samples were quenched in a sample pot with excess methanol for cocatalyst deactivation and given a small nitrogen purge at 40 °C to remove gross amounts of the light hydrocarbons.
  • Methanol was fed to the hold vessel to neutralize catalyst/cocatalyst based on the amount of alkyl fed to the reactor in the range of methanol-to-alkyl molar ratio of 1.4 - 1.5.
  • the product in the hold vessel was also treated with 4 phr of a liquid stabilizer before discharge to a fluidized bed purger.
  • the stabilizer contained 0.63 wt % Vitamin E; 5 wt % di-tridecyl thiodipropionate; 30 wt % HyBase® C-400 (a calcium additive); and 0.13 wt % Plastistab® 2116 (a barium tracer), in a mixture of mineral oil and soybean oil.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Health & Medical Sciences (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Engineering & Computer Science (AREA)
  • Combustion & Propulsion (AREA)
  • Materials Engineering (AREA)
  • Polymerisation Methods In General (AREA)
  • Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
  • Compositions Of Macromolecular Compounds (AREA)

Claims (10)

  1. Procédé post-réacteur permettant d'améliorer la robustesse de particules de polymère contenant au moins 0,3 % en poids d'un matériau particulaire inerte et mélangées à un monomère n'ayant pas réagi, lequel procédé comporte le fait d'introduire le polymère contenant au moins 0,3 % en poids de matériau particulaire inerte et le monomère n'ayant pas réagi dans un récipient de polissage où le polymère est fluidisé à l'aide d'un gaz inerte, où la température du polymère vaut de 20 à 100 °C et la température du gaz de fluidisation vaut de 20 à 150 °C, alors que la température régnant dans le récipient de polissage vaut de 50 à 100 °C, que la pression régnant dans le récipient de polissage vaut de -13,8 à 345 kPa (-2 à 50 psi), que la vitesse superficielle du gaz vaut de 0,18 à 0,91 m/s (0,6 à 3 ft/s), et que le temps de séjour du polymère vaut de 15 minutes à 8 heures.
  2. Procédé conforme à la revendication 1, dans lequel on met les particules de polymère en contact avec au moins un agent choisi parmi un inhibiteur de formation de gel, un désactivateur de catalyseur et un stabilisant.
  3. Procédé conforme à la revendication 1 ou 2, dans lequel on élimine au moins une partie du monomère n'ayant pas réagi.
  4. Procédé conforme à l'une des revendications précédentes, dans lequel on purge ultérieurement les particules de polymère.
  5. Procédé conforme à la revendication 4, dans lequel on met les particules de polymère, une fois qu'elles sont sorties du récipient de polissage, en contact avec de l'air humide, dans un ou plusieurs appareils de purge en lit fluidisé.
  6. Procédé conforme à l'une des revendications précédentes, dans lequel, dans l'appareil de polissage en lit fluidisé, le produit est fluidisé à une température de 50 à 80 °C pendant 1 à 5 heures.
  7. Procédé conforme à l'une des revendications précédentes, dans lequel le matériau particulaire inerte est choisi dans l'ensemble constitué par du noir de carbone, de la silice, de l'argile, du talc, et leurs mélanges.
  8. Procédé conforme à l'une des revendications précédentes, dans lequel les particules de polymère contenant au moins 0,3 % en poids de matériau particulaire inerte sont produites selon un procédé de polymérisation en phase gazeuse.
  9. Procédé conforme à l'une des revendications précédentes, dans lequel le polymère produit est choisi dans l'ensemble constitué par les suivants :
    caoutchouc IR (polyisoprène)
    caoutchouc BR (polybutadiène)
    caoutchouc SBR (polymère de butadiène copolymérisé avec du styrène)
    caoutchouc nitrile (polymère de butadiène copolymérisé avec de l'acrylonitrile)
    caoutchouc butyl (polymère d'isobutène copolymérisé avec de l'isoprène)
    caoutchouc EPM (polymère d'éthylène copolymérisé avec du propylène)
    caoutchouc EPDM (polymère d'éthylène copolymérisé avec du propylène et un diène comme de l'hexadiène, du dicyclopentadiène ou de l'éthylidène-norbornène)
    copolymères d'éthylène et d'une alpha-oléfine en C3-12
    homopolymères d'une alpha-oléfine en C2-18
    terpolymères d'éthylène, d'une alpha-oléfine en C3-12 et d'un diène (non conjugué de préférence)
    Néoprène® (polychloroprène)
    caoutchouc silicone (polydiméthylsiloxane)
    copolymères d'éthylène et de vinyltriméthoxysilane
    copolymères d'éthylène et d'un ou plusieurs des comonomères acrylonitrile, esters d'acide maléique, acétate de vinyle, esters d'acide acrylique ou méthacrylique, etc.
    copolymères de butadiène et d'isoprène
    polystyrène
    terpolymères de styrène, butadiène et isoprène
    caoutchouc chlorobutyl (copolymère chloré d'isobutène et d'isoprène)
    caoutchouc bromobutyl (copolymère bromé d'isobutène et d'isoprène)
    copolymère bromé d'isobutène et de para-méthylstyrène
    polyéthylène chloré et polyéthylène chlorosulfoné.
  10. Procédé permettant d'éliminer en grande partie les fines présentes parmi des particules de polymère d'éthylène et d'alpha-oléfine, et éventuellement de diène, produites dans un réacteur de polymérisation en phase gazeuse en lit fluidisé, en présence d'un matériau particulaire inerte, lequel procédé comporte :
    a) le fait d'envoyer les particules de polymère sortant du réacteur de polymérisation en phase gazeuse en lit fluidisé, qui contiennent du matériau particulaire inerte, et le cas échéant, des résidus d'un ou de plusieurs monomères n'ayant pas réagi, dans une cuve de stockage de produit et de mettre ces particules de polymère en contact avec un gaz inerte, à une vitesse et à une température qui sont suffisantes pour que le monomère alpha-oléfine n'ayant pas réagi soit éliminé ;
    b) le fait de faire passer ces particules de polymère contenant du matériau particulaire inerte, d'où le monomère alpha-oléfine n'ayant pas réagi a été éliminé, dans un dispositif de tamisage et d'en éliminer les agglomérats dont le diamètre est supérieur à 1,27 cm (1/2 pouce) ;
    c) le fait d'introduire ces particules de polymère, d'où les agglomérats ont été éliminés, dans une zone de polissage où les particules de polymère sont chauffées à une température de 20 à 100 °C, où le monomère diène n'ayant pas réagi, s'il y en a, est en partie éliminé, et où les particules de polymère sont fluidisées à l'aide d'un gaz inerte chauffé à une température de 20 à 150 °C, alors que la pression régnant dans le récipient de polissage vaut de -13,8 à 345 kPa (-2 à 50 psi), que la vitesse superficielle du gaz vaut de 0,18 à 0,91 m/s (0,6 à 3 ft/s), et que le temps de séjour moyen des particules de polymère vaut de 15 minutes à 8 heures ;
    d) le fait d'envoyer les particules de polymère sortant dudit récipient de polissage dans au moins un récipient de purge en lit fluidisé, dans lequel lesdites particules de polymère sont laissées, pendant un laps de temps de 0,25 à 3 heures, en contact avec de l'air humide chauffé à une température de 60 à 150 °C, puis refroidies à une température de 35 à 45 °C ;
    e) et le fait de décharger lesdites particules de polymère dudit récipient de purge.
EP99930248A 1998-06-16 1999-06-14 Procede post-reacteur permettant de traiter des polymeres prepares par polymerisation en phase gazeuse en presence d'un materiau particulaire inerte Expired - Lifetime EP1088006B1 (fr)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
US98479 1998-06-16
US09/098,479 US6214903B1 (en) 1998-06-16 1998-06-16 Post-reactor process for treating polymers prepared in a gas phase polymerization in the presence of an inert particulate material
PCT/US1999/013402 WO1999065953A1 (fr) 1998-06-16 1999-06-14 Procede post-reacteur permettant de traiter des polymeres prepares par polymerisation en phase gazeuse en presence d'un materiau particulaire inerte

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EP1088006A1 EP1088006A1 (fr) 2001-04-04
EP1088006B1 true EP1088006B1 (fr) 2003-06-25

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Country Status (11)

Country Link
US (1) US6214903B1 (fr)
EP (1) EP1088006B1 (fr)
JP (1) JP2002518528A (fr)
KR (1) KR20010052872A (fr)
CN (1) CN1312822A (fr)
AT (1) ATE243715T1 (fr)
AU (1) AU4682699A (fr)
BR (1) BR9911232A (fr)
DE (1) DE69909088T2 (fr)
ES (1) ES2196825T3 (fr)
WO (1) WO1999065953A1 (fr)

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AU2002360862A1 (en) * 2002-01-15 2003-07-30 Advanced Elastomer Systems, L.P. Thermoplastic elastomers and process for making the same
EP1558651B1 (fr) * 2002-10-30 2009-02-25 INEOS Manufacturing Belgium NV Traitement de polymere
EP1591457A1 (fr) * 2004-04-30 2005-11-02 SOLVAY (Société Anonyme) Traitement de polyolefine permettant de separer des matieres volatiles
JP2008511689A (ja) * 2004-07-27 2008-04-17 ダウ グローバル テクノロジーズ インコーポレイティド 熱可塑性加硫物およびこれらの調製方法
US6987152B1 (en) 2005-01-11 2006-01-17 Univation Technologies, Llc Feed purification at ambient temperature
WO2007109877A1 (fr) * 2006-03-29 2007-10-04 Lanxess Inc. Procede de polymerisation pour la preparation de nanocomposites de caoutchouc butylique
CN100513431C (zh) * 2006-04-20 2009-07-15 中国石油化工股份有限公司 一种处理固态烯烃聚合物的方法
TW200936564A (en) * 2007-11-15 2009-09-01 Univation Tech Llc Methods for the removal of impurities from polymerization feed streams
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Publication number Publication date
ATE243715T1 (de) 2003-07-15
ES2196825T3 (es) 2003-12-16
CN1312822A (zh) 2001-09-12
JP2002518528A (ja) 2002-06-25
EP1088006A1 (fr) 2001-04-04
KR20010052872A (ko) 2001-06-25
DE69909088T2 (de) 2004-05-06
BR9911232A (pt) 2001-03-06
WO1999065953A1 (fr) 1999-12-23
US6214903B1 (en) 2001-04-10
DE69909088D1 (de) 2003-07-31
AU4682699A (en) 2000-01-05
WO1999065953A9 (fr) 2000-04-06

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